Method for facilitating the separation of nitroglycerin.



eeeri JISEISEQLB? VIEYEL, ti l? BfiRRIG-ERE-IEXDE, GERLMANY, ASS'EGNOR, BY MESIIE ASSIGNIWHQNTS,

Ti FUHEHQ'ZSCHIE DYNAMITFABRIK, OF COLOGNE, GERMIANY.

METHOD FOR FACILITATIITG THE SEPARATION OF NITROGLYCEB-IN.

have been used for the manufacture of the some, thereby minimizing the element of danger which is present in the separation.

heen proposed to add certain sulr during the production of the nitro- 'erin in ord r to facilitate the separation the nitro yeerin, the substances suggested l.-

paranin oil, hydrofluoric acid or fluoride soluble silicates of the alkalis or alkaline earths. The use of pcratlin oil is, however,v disadvantageous inasmuch as an un'csirabl mud is formed on the surface toe niti glycerin in the separating tank, sses in the second seperation. sons paraffin. oil is only used in the degree 01 separation has lv' poor. The use of soluble l alis or alkaline earths has not entirely effective tarcl the separation owing ing character. In the mani in iiofiuoric acid and fluoride previously used induce the have been separation of the nitroglycerin, these substances used to remove the emulsified silicious compounds present in the acids used for trea ing the glycerin, on the vi theory that the presence of such silicious eompouni of thacids. was th e'fore understood that the use of r drotluo acid or fluorids would be advantageous only in case of the presence of such silicious compounds. I ll,'': found that in those cases in which sil' or silicious compounds are absent, the addition of chemically pure sodium fiuorid or hydrofluoric acid is always ineffective,

that in,all cases the best effect is obtained when cure is taken to produce a quantity of gaseous silicon fluorid by the presence of insoluble silicious compounds.

Specification of Letters Patent.

Patented lilny .l. 'l Tl ill 0,

Application filed Hovember 25, 1912. Serial No. 733,232

The production of gaseous silicon iiuorid results in loosening the mixture and opening the Way for the rise of the nitroglycerin, which has a lower specific gravity than the acids used for producing the same, and the use of insoluble compounds of silica to produce the silicon fluorid avoids any tendency to emulsificution which is present in the case of soluble silicon compounds. One Way of causing the liberation of silicon tluorid in this manner is by adding to the acids it mix ture of sodium fluorid and an insoluble silicious compound, such as silica or one of the insoluble silicates. The reaction which takes place is the following:

imir1+sio,+2n,so,=

siri eu so en o.

Care should he token to add the lluorid and silicious compound for the reason that they are added too soon the air agitation will. drive off the silicon liuorid before the formation of the nitroglycerin, and if they are added too late there Will not sufficient time to allow the silicon iluorid to form.

In cerying out the process it has been found advantageous to mix l on fluorid with about 8 to 33% of its own Weight fine, Washed, light lrieselguhr, end i" about 20 of this mixture to 100 the glycerin at from five to six ininut s before the end the nitration. It will he found, in carrying out the process in this manner, that the time for the separation 01' the nitroglycerin will be about one-third of its normal duration.

It will be understood that the process may substance of this character which may be used is sodium fluosilicate; In carrying out my invention with this compound, the rcaction is as follow In usingsodium fluosilicute, from 10 to g. thereof should he added to 100 kg. of glycerin. It will be noted that in this reaction there is an c'Xoess of hydrofluoric: acid formed and it is therefore advisable to add at the proper time aboi e in detail, I Wish it to. the sodium fluosilicate about 10% of silica, preferably in the form of kieselguhr. hen using silica with the sodiumfluosili- Cate, even a smaller quantity of the materials may be added to bring about-the separation of the nitroglycerin in the same period of time.

' While I have described my invention .to be understood that many changes may be made therein Without departing from the spirit thereof.

I clalmz 1. The method of facilitating the separation of a mixture of liquids containing nitroglycerin and an acid, which comprises generating silicon fiuorid in said liquids by the addition of a fiuorid and an insoluble silicious compound.

generating silicon and an acid Which comprises said liquids by. the addi- 2., The methodof facilitating the separation oi a mixture of liquids having different specific gravitiesj, containing nitroglycerin generating silicon fiuorid in tion of a fluorid compound.

The method of facilitating the separation of a mixture of liquids containing nitroglycerin and an acid, which. comprises fluorid in said liquids by the addition of sodium fluorid and an insoluble silicious compound.

a. The method of facilitating the separation of a mixture of liquids having differand an insoluble silicious 'ent specific gravities,

- tion of a mixture ent specific gravities, erin and an acid, which comprises generating silicon fiuorid in said liquids by the ad dition of sodium iluorid and an insoluble silicious compound.

- -5. The method of facilitating the separa tion of a mixture of liquids containing nitroglycerin and an acid, which comprises generating silicon fluorid-in said liquids by containing nitroglycthe addition of a fiuorid and insoluble silica. 4

6. The method of facilitating the separation of a mixture of liquids having differ containing nitroglycerm and an acid, which comprises generating silicon fiuorid in said liquids by the ad dition of sodium fluorid and insoluble silica.

7. The method of liquids containing nitroglycerin and 'an acid, which comprises generating silicon fluorid in said liquids by the addition of a fluorid and kieselguhin- 8. The method of facilitating the separation of a mixture of liquids having different specific gravities, containing nitroglycerin and an acid, which comprises generating;

silicon fiuorid in said liquids by the addition of sodium fluorid and kieselguhr.

In testimony thatI claim the foregoing I have hereunto set my hand.

RUDOLE' WEYEL.

Witnesses Louis VANDORY, KARL 'KNAPP.

of facilitating the separa- 

